US2694652A - Production of metallic titanium - Google Patents

Production of metallic titanium Download PDF

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Publication number
US2694652A
US2694652A US20594A US2059448A US2694652A US 2694652 A US2694652 A US 2694652A US 20594 A US20594 A US 20594A US 2059448 A US2059448 A US 2059448A US 2694652 A US2694652 A US 2694652A
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titanium
tetraiodide
metallic
production
triiodide
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US20594A
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Alfred C Loonam
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Chilean Nitrate Corp
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Chilean Nitrate Corp
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/129—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds by dissociation, e.g. thermic dissociation of titanium tetraiodide, or by electrolysis or with the use of an electric arc

Definitions

  • This invention relates to the production of metallic titanium and has for an object the provision of an improved method or process for producing high-purity metallic titanium. More particularly, the invention contemplates the provision of an improved method or process for producing high-purity metallic titanium by dissociation of titanium tetraiodide.
  • metallic titanium of high purity is produced by contacting titanium tetraiodide with a heated surface maintained at a temperature in the range 1100 C. to 1700 C.
  • Contact of the titanium tetraiodide with the heated surface results in dissociation of the iodine and titanium of the titanium tetraiodide with deposition of the titanium on the heated surface and with the production of a gaseous product containing the iodine in vapor form.
  • Titanium or tungsten or some other suitable metal is employed in forming the heated surface.
  • the titanium tetraiodide employed is formed by contacting iodine in vapor form with crude metallic titanium.
  • the dissociation operation is carried out in a closed vessel or chamber under high vacuum, and the amount of titamum contained 1n each unit of volume of the vessel or chamber, and, consequently, the amount of titanium available for deposition from each .unit of titanium tetraiodide vapor therein, is relatively small.
  • the present invention provides a method of increasing the eificiency of the deposition operation by making available for deposition a greater amount of titanium is each unit of volume of the deposition vessel or cham-
  • the invention utilizes that property of titanium triiodide which permits it to remain stable at elevated temperatures in the presence of titanium tetraiodide, and, in utilizing that property, the invention employs, in the deposition vessel or chamber a mixture of titanium triiodide and titanium tetraiodide instead of titanium tetraiodide alone.
  • the resulting gaseous product is contacted with crude titanium metal such as scrap metal at a temperature in the range 600 C. to 1000 C. to produce a stable mixture of titates Patent 2,694,652 Patented Nov. 16, 1954 'ice tanium tetraiodide and titanium triiodide
  • the miX- ture is contacted with a heated surface at a temperature in the range 1100 C. to 1700 C. to produce metallic titanium and a gaseous product containing elemental iodine.
  • the gaseous products containing elemental iodine are utilized in the production of additional titanium iodides.
  • a gaseous product comprising elemental iodine preferably is contacted with titanium carbide at a temperature of about 1100 C. to form a gaseous product containing titanium tetraiodide which is contacted with metallic titanium at a temperature in the range 600 C. to 1000 C. to convert a portion of the titanium tetraiodide to titanium triiodide to regenerate the gaseous product containing titanium tetraiodide and titanium triiodide for re-use in the deposition operation.
  • the method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material which comprises contacting a gaseous product comprising titanium tetraiodide and titanium triiodide with a heater refractory surface maintained at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide and the titanium triiodide with the production and deposition of metallic titanium on the refractory surface and the production of a gaseous product comprising elemental iodine, reacting the elemental iodine thus produced with titanium carbide at a temperature of about 1100 C. to form a.
  • the method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material which comprises contacting a gaseous product comprising titanium tetraiodide and titanium triiodide with a heated body of metallic titanium maintained at a temperature in the range 1100 C. to 1700 C. to eflect dissociation of the titanium tetraiodide and the titanium triiodide with the production and deposition of metallic titanium on the body of metallic titanium and the production of a gaseous product comprising elemental iodine, reacting the elemental iodine thus produced with titanium carbide at a temperature of about 1100 C.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Carbon And Carbon Compounds (AREA)

Description

United PRODUCTION OF METALLIC TITANIUM No Drawing. Application April 12, 1948, Serial No. 20,594
2 Claims. (Cl. 117-107) This invention relates to the production of metallic titanium and has for an object the provision of an improved method or process for producing high-purity metallic titanium. More particularly, the invention contemplates the provision of an improved method or process for producing high-purity metallic titanium by dissociation of titanium tetraiodide.
According to some heretofore customary procedures, metallic titanium of high purity is produced by contacting titanium tetraiodide with a heated surface maintained at a temperature in the range 1100 C. to 1700 C. Contact of the titanium tetraiodide with the heated surface results in dissociation of the iodine and titanium of the titanium tetraiodide with deposition of the titanium on the heated surface and with the production of a gaseous product containing the iodine in vapor form. Titanium or tungsten or some other suitable metal is employed in forming the heated surface.
The titanium tetraiodide employed is formed by contacting iodine in vapor form with crude metallic titanium. The dissociation operation is carried out in a closed vessel or chamber under high vacuum, and the amount of titamum contained 1n each unit of volume of the vessel or chamber, and, consequently, the amount of titanium available for deposition from each .unit of titanium tetraiodide vapor therein, is relatively small.
The present invention provides a method of increasing the eificiency of the deposition operation by making available for deposition a greater amount of titanium is each unit of volume of the deposition vessel or cham- The invention utilizes that property of titanium triiodide which permits it to remain stable at elevated temperatures in the presence of titanium tetraiodide, and, in utilizing that property, the invention employs, in the deposition vessel or chamber a mixture of titanium triiodide and titanium tetraiodide instead of titanium tetraiodide alone.
When the mixture of iodides contacts the heated surface, the tetraiodide is dissociated, disturbing the equilibrlum and permitting progressive dissociation of the triiodide in accordance with the following equations:
In a preferred process of the invention, iodine in vapor form 1s contacted with titanium carbide at an elevated temperature such, for example, as 1100 C., to produce a gaseous product comprising titanium tetraiodide, the resulting gaseous product is contacted with crude titanium metal such as scrap metal at a temperature in the range 600 C. to 1000 C. to produce a stable mixture of titates Patent 2,694,652 Patented Nov. 16, 1954 'ice tanium tetraiodide and titanium triiodide, and the miX- ture is contacted with a heated surface at a temperature in the range 1100 C. to 1700 C. to produce metallic titanium and a gaseous product containing elemental iodine.
The gaseous products containing elemental iodine are utilized in the production of additional titanium iodides. A gaseous product comprising elemental iodine preferably is contacted with titanium carbide at a temperature of about 1100 C. to form a gaseous product containing titanium tetraiodide which is contacted with metallic titanium at a temperature in the range 600 C. to 1000 C. to convert a portion of the titanium tetraiodide to titanium triiodide to regenerate the gaseous product containing titanium tetraiodide and titanium triiodide for re-use in the deposition operation.
I claim:
1. The method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material which comprises contacting a gaseous product comprising titanium tetraiodide and titanium triiodide with a heater refractory surface maintained at a temperature in the range 1100 C. to 1700 C. to effect dissociation of the titanium tetraiodide and the titanium triiodide with the production and deposition of metallic titanium on the refractory surface and the production of a gaseous product comprising elemental iodine, reacting the elemental iodine thus produced with titanium carbide at a temperature of about 1100 C. to form a. gaseous product containing titanium tetraiodide, reacting the titanium tetraiodide thus produced with metallic titanium at a temperature in the range 600 C. to 1100 C. to convert a portion of the titanium tetraiodide to titanium triiodide, and passing the regenerated titanium tetraiodide and titanium triiodide in contact with the refractory surface for the production and deposition of additional metallic titanium.
2. The method of recovering titanium in the form of a high-purity metallic product from crude titanium-bearing material which comprises contacting a gaseous product comprising titanium tetraiodide and titanium triiodide with a heated body of metallic titanium maintained at a temperature in the range 1100 C. to 1700 C. to eflect dissociation of the titanium tetraiodide and the titanium triiodide with the production and deposition of metallic titanium on the body of metallic titanium and the production of a gaseous product comprising elemental iodine, reacting the elemental iodine thus produced with titanium carbide at a temperature of about 1100 C. to form a gaseous product containing titanium tetraiodide, reacting the titanium tetraiodide thus produced with a crude titanium-bearing material at a temperature in the the range 600 C. to 1100 C. to convert a portion of the titanium tetraiodide to titanium triiodide, and passing the regenerated titanium tetraiodide and titanium tri iodide in contact with the heated body of metallic titanium for the production and deposition of additional quantities of metallic titanium.
References Cited in the file of this patent UNITED STATES PATENTS Number Name Date 1,497,417 Weber June 10, 1924 1,671,213 Van Arkel et a1 May 29, 1928 1,891,124 Van Arkel et al Dec. 13, 1932 2,393,264 Rentschler et a1. Jan. 22, 1946 2,519,385 Loonam Aug. 22, 1950

Claims (1)

1. THE METHOD OF RECOVERING TITANIUM IN THE FORM OF A HIGH-PURITY METALLIC PRODUCT FROM CRUDE TITANIUM-BEARING MATERIAL WHICH COMPRISES CONTACTING A GASEOUS PRODUCT COMPRISING TITANIUM TETRAIODIDE AND TITANIUM TRIIODIDE WITH A HEATER REFRACTORY SURFACE MAINTAINED AT A TEMPERATURE IN THE RANGE 1100* C. TO 1700* C. TO EFFECT DISSOCIATION OF THE TITANIUM TETRAIODIDE AND THE TITANIUM TRIIODIDE WITH THE PRODUCTION AND DEPOSITION OF METALLIC TITANIUM ON THE REFRACTORY SURFACE AND THE PRODUCTION OF A GASEOUS PRODUCT COMPRISING ELEMENTAL IODINE, REACTING THE ELEMENTAL IODINE THUS PRODUCED WITH TITANIUM CARBIDE AT A TEMPERATURE OF ABOUT 1100* C. TO FORM A GASEOUS PRODUCT CONTAINING TITANIUM TETRAIODIDE, REACTING THE TITANIUM TETRAIODIDE THUS PRODUCED WITH METALLIC TITANIUM AT A TEMPERATUR IN THE RANGE 600* C. TO 1100* C. TO CONVERT A PORTION OF THE TITANIUM TETRAIODIDE TO TITANIUM TRIIODIDE, AND PASSING THE REGENERATED TITANIUM TETRAIODIDE AND TITANIUM TRIIODIDE IN CONTACT WITH THE REFRACTORY SURFACE OF THE PRODUCTION AND DEPOSITION OF ADDITIONAL METALLIC TITANIUM.
US20594A 1948-04-12 1948-04-12 Production of metallic titanium Expired - Lifetime US2694652A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2783142A (en) * 1952-08-14 1957-02-26 Nat Res Corp Method of producing titanium
US2809108A (en) * 1952-08-14 1957-10-08 Nat Res Corp Method of producing titanium
US2890952A (en) * 1955-11-04 1959-06-16 Lummus Co Method of refining metals
US2895852A (en) * 1954-11-16 1959-07-21 Chilean Nitrate Sales Corp Titanium metallurgy
US2905573A (en) * 1957-12-10 1959-09-22 Union Carbide Corp Method of gas plating
US2925392A (en) * 1956-04-02 1960-02-16 Exxon Research Engineering Co Catalyst and preparation thereof
US3049440A (en) * 1959-07-28 1962-08-14 Chilean Nitrate Sales Corp Process and apparatus for the vapor deposition of metals

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1497417A (en) * 1919-03-31 1924-06-10 Henry C P Weber Process of coating metals
US1671213A (en) * 1925-03-14 1928-05-29 Philips Nv Process of precipitaing metals on an incandescent body
US1891124A (en) * 1928-06-14 1932-12-13 Philips Nv Process of precipitating metals on an incandescent body
US2393264A (en) * 1942-09-23 1946-01-22 Westinghouse Electric Corp Photoelectric device and the manufacture thereof
US2519385A (en) * 1948-04-12 1950-08-22 Chilean Nitrate Sales Corp Production of titanium tetraiodide

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1497417A (en) * 1919-03-31 1924-06-10 Henry C P Weber Process of coating metals
US1671213A (en) * 1925-03-14 1928-05-29 Philips Nv Process of precipitaing metals on an incandescent body
US1891124A (en) * 1928-06-14 1932-12-13 Philips Nv Process of precipitating metals on an incandescent body
US2393264A (en) * 1942-09-23 1946-01-22 Westinghouse Electric Corp Photoelectric device and the manufacture thereof
US2519385A (en) * 1948-04-12 1950-08-22 Chilean Nitrate Sales Corp Production of titanium tetraiodide

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2783142A (en) * 1952-08-14 1957-02-26 Nat Res Corp Method of producing titanium
US2809108A (en) * 1952-08-14 1957-10-08 Nat Res Corp Method of producing titanium
US2895852A (en) * 1954-11-16 1959-07-21 Chilean Nitrate Sales Corp Titanium metallurgy
US2890952A (en) * 1955-11-04 1959-06-16 Lummus Co Method of refining metals
US2925392A (en) * 1956-04-02 1960-02-16 Exxon Research Engineering Co Catalyst and preparation thereof
US2905573A (en) * 1957-12-10 1959-09-22 Union Carbide Corp Method of gas plating
US3049440A (en) * 1959-07-28 1962-08-14 Chilean Nitrate Sales Corp Process and apparatus for the vapor deposition of metals

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